Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Wayne Gladfelter' 'Benjamin E. Kucera' 'Bing Luo' _publ_contact_author_name 'Wayne Gladfelter' _publ_contact_author_address ; Department of Chemistry University of Minnesota 207 Pleasant Street Minneapolis 55455 UNITED STATES OF AMERICA ; _publ_contact_author_email GLADFELT@CHEM.UMN.EDU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Hydrido and chloro gallium and aluminum complexes with tridentate bis(2-dimethylaminoethyl)amide ; data_04265n _database_code_depnum_ccdc_archive 'CCDC 608294' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 04265n _chemical_melting_point ? _chemical_formula_moiety 'C8 H20 Cl2 Ga N3' _chemical_formula_sum 'C8 H20 Cl2 Ga N3' _chemical_formula_weight 298.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.1776(15) _cell_length_b 13.712(2) _cell_length_c 9.5000(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.516(2) _cell_angle_gamma 90.00 _cell_volume 1325.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3298 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 616 _exptl_absorpt_coefficient_mu 2.450 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.373 _exptl_absorpt_correction_T_max 0.542 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans per phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15458 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.55 _reflns_number_total 3048 _reflns_number_gt 2727 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+1.9786P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3048 _refine_ls_number_parameters 156 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0866 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.74582(4) 0.46422(2) 0.20032(3) 0.02887(10) Uani 1 1 d D . . Cl1 Cl 0.56457(10) 0.39123(8) 0.27346(11) 0.0547(3) Uani 1 1 d . A . Cl2 Cl 0.91792(11) 0.38720(9) 0.29091(13) 0.0650(3) Uani 1 1 d . A . C1 C 0.6650(7) 0.3066(5) -0.0301(8) 0.0533(14) Uani 0.575(4) 1 d PD A 1 H1A H 0.6655 0.2882 -0.1298 0.080 Uiso 0.575(4) 1 calc PR A 1 H1B H 0.5744 0.3178 -0.0001 0.080 Uiso 0.575(4) 1 calc PR A 1 H1C H 0.7040 0.2540 0.0263 0.080 Uiso 0.575(4) 1 calc PR A 1 C2 C 0.8782(6) 0.3787(5) -0.0613(8) 0.0537(14) Uani 0.575(4) 1 d PD A 1 H2A H 0.8757 0.3694 -0.1636 0.081 Uiso 0.575(4) 1 calc PR A 1 H2B H 0.9133 0.3199 -0.0161 0.081 Uiso 0.575(4) 1 calc PR A 1 H2C H 0.9347 0.4345 -0.0382 0.081 Uiso 0.575(4) 1 calc PR A 1 N1 N 0.7430(6) 0.3976(3) -0.0098(4) 0.0395(7) Uani 0.575(4) 1 d PD A 1 C3 C 0.6816(6) 0.4769(4) -0.0943(6) 0.0444(11) Uani 0.575(4) 1 d PD A 1 H3A H 0.5863 0.4798 -0.0748 0.053 Uiso 0.575(4) 1 calc PR A 1 H3B H 0.6929 0.4632 -0.1958 0.053 Uiso 0.575(4) 1 calc PR A 1 C4 C 0.7450(7) 0.5745(4) -0.0578(5) 0.0418(17) Uani 0.575(4) 1 d PD A 1 H4A H 0.8328 0.5798 -0.1012 0.050 Uiso 0.575(4) 1 calc PR A 1 H4B H 0.6897 0.6291 -0.0918 0.050 Uiso 0.575(4) 1 calc PR A 1 N2 N 0.7559(17) 0.5763(3) 0.0919(4) 0.035(2) Uani 0.575(4) 1 d PD A 1 C5 C 0.783(2) 0.6697(4) 0.1578(6) 0.048(3) Uani 0.575(4) 1 d PD A 1 H5A H 0.7028 0.7106 0.1580 0.057 Uiso 0.575(4) 1 calc PR A 1 H5B H 0.8524 0.7048 0.1057 0.057 Uiso 0.575(4) 1 calc PR A 1 C6 C 0.8286(5) 0.6490(3) 0.3085(5) 0.0612(12) Uani 0.575(4) 1 d PD A 1 H6A H 0.9188 0.6219 0.3093 0.073 Uiso 0.575(4) 1 calc PR A 1 H6B H 0.8280 0.7095 0.3652 0.073 Uiso 0.575(4) 1 calc PR A 1 N3 N 0.7351(3) 0.5775(2) 0.3655(3) 0.0419(6) Uani 1 1 d . A . C7 C 0.6013(4) 0.6186(3) 0.3721(5) 0.0596(11) Uani 1 1 d . . . H7A H 0.6025 0.6779 0.4298 0.089 Uiso 1 1 calc R A . H7B H 0.5419 0.5707 0.4141 0.089 Uiso 1 1 calc R . . H7C H 0.5705 0.6346 0.2768 0.089 Uiso 1 1 calc R . . C8 C 0.7735(5) 0.5465(4) 0.5093(4) 0.0645(12) Uani 1 1 d . . . H8A H 0.7642 0.6016 0.5742 0.097 Uiso 1 1 calc R A . H8B H 0.8651 0.5245 0.5094 0.097 Uiso 1 1 calc R . . H8C H 0.7165 0.4930 0.5395 0.097 Uiso 1 1 calc R . . C1' C 0.6154(7) 0.3805(7) -0.0637(10) 0.0533(14) Uani 0.425(4) 1 d PD A 5 H1'A H 0.6210 0.3571 -0.1609 0.080 Uiso 0.425(4) 1 calc PR A 5 H1'B H 0.5751 0.4454 -0.0628 0.080 Uiso 0.425(4) 1 calc PR A 5 H1'C H 0.5617 0.3354 -0.0087 0.080 Uiso 0.425(4) 1 calc PR A 5 C2' C 0.8037(9) 0.2860(6) 0.0090(10) 0.0537(14) Uani 0.425(4) 1 d PD A 5 H2'A H 0.8097 0.2577 -0.0854 0.081 Uiso 0.425(4) 1 calc PR A 5 H2'B H 0.7458 0.2457 0.0669 0.081 Uiso 0.425(4) 1 calc PR A 5 H2'C H 0.8914 0.2884 0.0523 0.081 Uiso 0.425(4) 1 calc PR A 5 N1' N 0.7494(7) 0.3861(4) -0.0011(4) 0.0395(7) Uani 0.425(4) 1 d PD A 5 C3' C 0.8334(7) 0.4511(5) -0.0853(8) 0.0444(11) Uani 0.425(4) 1 d PD A 5 H3'A H 0.8244 0.4343 -0.1862 0.053 Uiso 0.425(4) 1 calc PR A 5 H3'B H 0.9265 0.4420 -0.0572 0.053 Uiso 0.425(4) 1 calc PR A 5 C4' C 0.7938(10) 0.5575(5) -0.0627(6) 0.0418(17) Uani 0.425(4) 1 d PD A 5 H4'A H 0.8609 0.6020 -0.1015 0.050 Uiso 0.425(4) 1 calc PR A 5 H4'B H 0.7084 0.5713 -0.1094 0.050 Uiso 0.425(4) 1 calc PR A 5 N2' N 0.784(2) 0.5694(4) 0.0854(5) 0.035(2) Uani 0.425(4) 1 d PD A 5 C5' C 0.811(3) 0.6631(5) 0.1495(8) 0.048(3) Uani 0.425(4) 1 d PD A 5 H5'A H 0.7369 0.7083 0.1307 0.057 Uiso 0.425(4) 1 calc PR A 5 H5'B H 0.8915 0.6915 0.1091 0.057 Uiso 0.425(4) 1 calc PR A 5 C6' C 0.8286(5) 0.6490(3) 0.3085(5) 0.0612(12) Uani 0.425(4) 1 d PD A 5 H6'A H 0.9194 0.6266 0.3283 0.073 Uiso 0.425(4) 1 calc PR A 5 H6'B H 0.8162 0.7123 0.3565 0.073 Uiso 0.425(4) 1 calc PR A 5 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ga1 0.03365(17) 0.02194(15) 0.03101(16) 0.00177(12) -0.00126(15) -0.00058(14) Cl1 0.0545(6) 0.0546(6) 0.0553(6) -0.0020(5) 0.0125(4) -0.0243(5) Cl2 0.0587(6) 0.0727(7) 0.0634(6) 0.0038(6) -0.0137(5) 0.0315(5) C1 0.052(3) 0.048(3) 0.059(3) -0.022(3) -0.003(3) -0.009(3) C2 0.049(3) 0.050(3) 0.061(3) -0.025(3) 0.002(3) -0.001(3) N1 0.0371(15) 0.0341(15) 0.0473(15) -0.0164(12) 0.0005(14) 0.0004(15) C3 0.047(3) 0.055(3) 0.031(2) -0.009(2) -0.001(2) -0.001(2) C4 0.042(5) 0.048(3) 0.0351(18) 0.0086(18) 0.000(3) 0.000(3) N2 0.051(7) 0.0240(13) 0.0315(13) 0.0015(11) 0.0075(18) 0.001(2) C5 0.063(9) 0.0205(16) 0.060(2) -0.0011(16) 0.026(3) -0.001(3) C6 0.085(3) 0.040(2) 0.059(2) -0.0197(19) 0.019(2) -0.027(2) N3 0.0491(17) 0.0417(14) 0.0349(13) -0.0100(11) 0.0057(13) -0.0045(14) C7 0.067(3) 0.048(2) 0.064(3) -0.012(2) 0.020(2) 0.009(2) C8 0.080(3) 0.078(3) 0.0355(18) -0.0107(18) 0.001(2) -0.014(3) C1' 0.052(3) 0.048(3) 0.059(3) -0.022(3) -0.003(3) -0.009(3) C2' 0.049(3) 0.050(3) 0.061(3) -0.025(3) 0.002(3) -0.001(3) N1' 0.0371(15) 0.0341(15) 0.0473(15) -0.0164(12) 0.0005(14) 0.0004(15) C3' 0.047(3) 0.055(3) 0.031(2) -0.009(2) -0.001(2) -0.001(2) C4' 0.042(5) 0.048(3) 0.0351(18) 0.0086(18) 0.000(3) 0.000(3) N2' 0.051(7) 0.0240(13) 0.0315(13) 0.0015(11) 0.0075(18) 0.001(2) C5' 0.063(9) 0.0205(16) 0.060(2) -0.0011(16) 0.026(3) -0.001(3) C6' 0.085(3) 0.040(2) 0.059(2) -0.0197(19) 0.019(2) -0.027(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 N2' 1.852(3) . ? Ga1 N2 1.854(3) . ? Ga1 N1' 2.193(3) . ? Ga1 N1 2.195(3) . ? Ga1 N3 2.211(3) . ? Ga1 Cl2 2.2129(10) . ? Ga1 Cl1 2.2159(10) . ? C1 N1 1.491(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.487(7) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? N1 C3 1.486(7) . ? C3 C4 1.524(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N2 1.425(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? N2 C5 1.451(5) . ? C5 C6 1.528(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N3 1.473(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? N3 C7 1.476(5) . ? N3 C8 1.480(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C1' N1' 1.485(7) . ? C1' H1'A 0.9800 . ? C1' H1'B 0.9800 . ? C1' H1'C 0.9800 . ? C2' N1' 1.482(7) . ? C2' H2'A 0.9800 . ? C2' H2'B 0.9800 . ? C2' H2'C 0.9800 . ? N1' C3' 1.476(7) . ? C3' C4' 1.529(7) . ? C3' H3'A 0.9900 . ? C3' H3'B 0.9900 . ? C4' N2' 1.421(6) . ? C4' H4'A 0.9900 . ? C4' H4'B 0.9900 . ? N2' C5' 1.446(5) . ? C5' H5'A 0.9900 . ? C5' H5'B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2' Ga1 N2 9.5(13) . . ? N2' Ga1 N1' 82.0(2) . . ? N2 Ga1 N1' 85.3(2) . . ? N2' Ga1 N1 77.8(2) . . ? N2 Ga1 N1 80.78(16) . . ? N1' Ga1 N1 5.0(2) . . ? N2' Ga1 N3 83.3(2) . . ? N2 Ga1 N3 79.37(17) . . ? N1' Ga1 N3 164.46(17) . . ? N1 Ga1 N3 159.59(15) . . ? N2' Ga1 Cl2 115.6(8) . . ? N2 Ga1 Cl2 124.3(5) . . ? N1' Ga1 Cl2 94.97(18) . . ? N1 Ga1 Cl2 99.14(15) . . ? N3 Ga1 Cl2 95.93(9) . . ? N2' Ga1 Cl1 135.7(8) . . ? N2 Ga1 Cl1 126.8(5) . . ? N1' Ga1 Cl1 94.20(18) . . ? N1 Ga1 Cl1 95.35(14) . . ? N3 Ga1 Cl1 92.75(9) . . ? Cl2 Ga1 Cl1 108.71(5) . . ? C3 N1 C2 109.6(5) . . ? C3 N1 C1 108.8(4) . . ? C2 N1 C1 107.7(4) . . ? C3 N1 Ga1 100.9(3) . . ? C2 N1 Ga1 111.5(4) . . ? C1 N1 Ga1 117.9(4) . . ? N1 C3 C4 110.1(4) . . ? N1 C3 H3A 109.6 . . ? C4 C3 H3A 109.6 . . ? N1 C3 H3B 109.6 . . ? C4 C3 H3B 109.6 . . ? H3A C3 H3B 108.1 . . ? N2 C4 C3 105.8(4) . . ? N2 C4 H4A 110.6 . . ? C3 C4 H4A 110.6 . . ? N2 C4 H4B 110.6 . . ? C3 C4 H4B 110.6 . . ? H4A C4 H4B 108.7 . . ? C4 N2 C5 117.3(4) . . ? C4 N2 Ga1 122.4(3) . . ? C5 N2 Ga1 120.2(3) . . ? N2 C5 C6 107.1(5) . . ? N2 C5 H5A 110.3 . . ? C6 C5 H5A 110.3 . . ? N2 C5 H5B 110.3 . . ? C6 C5 H5B 110.3 . . ? H5A C5 H5B 108.5 . . ? N3 C6 C5 106.1(6) . . ? N3 C6 H6A 110.5 . . ? C5 C6 H6A 110.5 . . ? N3 C6 H6B 110.5 . . ? C5 C6 H6B 110.5 . . ? H6A C6 H6B 108.7 . . ? C6 N3 C7 111.2(3) . . ? C6 N3 C8 111.3(3) . . ? C7 N3 C8 107.9(3) . . ? C6 N3 Ga1 99.8(2) . . ? C7 N3 Ga1 110.5(2) . . ? C8 N3 Ga1 116.1(2) . . ? N3 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3' N1' C2' 112.2(5) . . ? C3' N1' C1' 110.4(5) . . ? C2' N1' C1' 108.6(5) . . ? C3' N1' Ga1 101.1(3) . . ? C2' N1' Ga1 113.9(4) . . ? C1' N1' Ga1 110.6(5) . . ? N1' C3' C4' 110.2(5) . . ? N1' C3' H3'A 109.6 . . ? C4' C3' H3'A 109.6 . . ? N1' C3' H3'B 109.6 . . ? C4' C3' H3'B 109.6 . . ? H3'A C3' H3'B 108.1 . . ? N2' C4' C3' 105.6(6) . . ? N2' C4' H4'A 110.6 . . ? C3' C4' H4'A 110.6 . . ? N2' C4' H4'B 110.6 . . ? C3' C4' H4'B 110.6 . . ? H4'A C4' H4'B 108.7 . . ? C4' N2' C5' 120.3(6) . . ? C4' N2' Ga1 120.7(4) . . ? C5' N2' Ga1 118.9(5) . . ? N2' C5' H5'A 109.9 . . ? N2' C5' H5'B 109.9 . . ? H5'A C5' H5'B 108.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2' Ga1 N1 C3 -37.7(9) . . . . ? N2 Ga1 N1 C3 -28.5(6) . . . . ? N1' Ga1 N1 C3 175(3) . . . . ? N3 Ga1 N1 C3 -15.0(7) . . . . ? Cl2 Ga1 N1 C3 -152.1(3) . . . . ? Cl1 Ga1 N1 C3 97.9(3) . . . . ? N2' Ga1 N1 C2 78.6(9) . . . . ? N2 Ga1 N1 C2 87.8(7) . . . . ? N1' Ga1 N1 C2 -69(3) . . . . ? N3 Ga1 N1 C2 101.3(6) . . . . ? Cl2 Ga1 N1 C2 -35.8(4) . . . . ? Cl1 Ga1 N1 C2 -145.7(4) . . . . ? N2' Ga1 N1 C1 -156.0(9) . . . . ? N2 Ga1 N1 C1 -146.8(7) . . . . ? N1' Ga1 N1 C1 57(3) . . . . ? N3 Ga1 N1 C1 -133.3(5) . . . . ? Cl2 Ga1 N1 C1 89.7(5) . . . . ? Cl1 Ga1 N1 C1 -20.3(5) . . . . ? C2 N1 C3 C4 -71.6(5) . . . . ? C1 N1 C3 C4 170.8(5) . . . . ? Ga1 N1 C3 C4 46.1(5) . . . . ? N1 C3 C4 N2 -44.2(10) . . . . ? C3 C4 N2 C5 -165.3(12) . . . . ? C3 C4 N2 Ga1 18.1(14) . . . . ? N2' Ga1 N2 C4 77.1(16) . . . . ? N1' Ga1 N2 C4 8.1(12) . . . . ? N1 Ga1 N2 C4 6.1(11) . . . . ? N3 Ga1 N2 C4 -169.2(13) . . . . ? Cl2 Ga1 N2 C4 100.9(12) . . . . ? Cl1 Ga1 N2 C4 -83.7(12) . . . . ? N2' Ga1 N2 C5 -99(3) . . . . ? N1' Ga1 N2 C5 -168.5(14) . . . . ? N1 Ga1 N2 C5 -170.4(14) . . . . ? N3 Ga1 N2 C5 14.3(13) . . . . ? Cl2 Ga1 N2 C5 -75.6(14) . . . . ? Cl1 Ga1 N2 C5 99.8(13) . . . . ? C4 N2 C5 C6 -164.1(12) . . . . ? Ga1 N2 C5 C6 12.6(18) . . . . ? N2 C5 C6 N3 -46.6(14) . . . . ? C5 C6 N3 C7 -63.2(7) . . . . ? C5 C6 N3 C8 176.5(6) . . . . ? C5 C6 N3 Ga1 53.4(6) . . . . ? N2' Ga1 N3 C6 -29.2(8) . . . . ? N2 Ga1 N3 C6 -37.9(6) . . . . ? N1' Ga1 N3 C6 -48.4(8) . . . . ? N1 Ga1 N3 C6 -51.5(6) . . . . ? Cl2 Ga1 N3 C6 86.0(3) . . . . ? Cl1 Ga1 N3 C6 -164.9(3) . . . . ? N2' Ga1 N3 C7 87.9(8) . . . . ? N2 Ga1 N3 C7 79.2(6) . . . . ? N1' Ga1 N3 C7 68.7(8) . . . . ? N1 Ga1 N3 C7 65.6(6) . . . . ? Cl2 Ga1 N3 C7 -156.9(2) . . . . ? Cl1 Ga1 N3 C7 -47.8(2) . . . . ? N2' Ga1 N3 C8 -148.9(8) . . . . ? N2 Ga1 N3 C8 -157.6(6) . . . . ? N1' Ga1 N3 C8 -168.1(7) . . . . ? N1 Ga1 N3 C8 -171.2(5) . . . . ? Cl2 Ga1 N3 C8 -33.7(3) . . . . ? Cl1 Ga1 N3 C8 75.4(3) . . . . ? N2' Ga1 N1' C3' 23.9(9) . . . . ? N2 Ga1 N1' C3' 32.8(6) . . . . ? N1 Ga1 N1' C3' 56(3) . . . . ? N3 Ga1 N1' C3' 43.1(10) . . . . ? Cl2 Ga1 N1' C3' -91.3(4) . . . . ? Cl1 Ga1 N1' C3' 159.5(4) . . . . ? N2' Ga1 N1' C2' 144.3(10) . . . . ? N2 Ga1 N1' C2' 153.3(7) . . . . ? N1 Ga1 N1' C2' 176(4) . . . . ? N3 Ga1 N1' C2' 163.6(6) . . . . ? Cl2 Ga1 N1' C2' 29.2(5) . . . . ? Cl1 Ga1 N1' C2' -80.1(5) . . . . ? N2' Ga1 N1' C1' -93.0(9) . . . . ? N2 Ga1 N1' C1' -84.1(7) . . . . ? N1 Ga1 N1' C1' -61(3) . . . . ? N3 Ga1 N1' C1' -73.8(10) . . . . ? Cl2 Ga1 N1' C1' 151.8(5) . . . . ? Cl1 Ga1 N1' C1' 42.6(5) . . . . ? C2' N1' C3' C4' -165.8(6) . . . . ? C1' N1' C3' C4' 73.0(7) . . . . ? Ga1 N1' C3' C4' -44.1(6) . . . . ? N1' C3' C4' N2' 47.8(12) . . . . ? C3' C4' N2' C5' 150(2) . . . . ? C3' C4' N2' Ga1 -26.4(19) . . . . ? N2 Ga1 N2' C4' -108(4) . . . . ? N1' Ga1 N2' C4' 1.8(16) . . . . ? N1 Ga1 N2' C4' -0.9(16) . . . . ? N3 Ga1 N2' C4' -173.1(18) . . . . ? Cl2 Ga1 N2' C4' 93.5(17) . . . . ? Cl1 Ga1 N2' C4' -86.1(19) . . . . ? N2 Ga1 N2' C5' 75.1(19) . . . . ? N1' Ga1 N2' C5' -175(2) . . . . ? N1 Ga1 N2' C5' -178(2) . . . . ? N3 Ga1 N2' C5' 10.2(19) . . . . ? Cl2 Ga1 N2' C5' -83(2) . . . . ? Cl1 Ga1 N2' C5' 97.3(19) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.763 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.070 # Attachment 'H2Al(NL2).cif' data_04264n _database_code_depnum_ccdc_archive 'CCDC 608295' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 04264 _chemical_melting_point ? _chemical_formula_moiety 'C8 H22 Al N3' _chemical_formula_sum 'C8 H22 Al N3' _chemical_formula_weight 187.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.9945(8) _cell_length_b 11.7842(9) _cell_length_c 9.3014(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1205.10(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2834 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.032 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 0.131 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9496 _exptl_absorpt_correction_T_max 0.9557 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans per phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12992 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0089 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.50 _reflns_number_total 1385 _reflns_number_gt 1280 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+0.3431P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1385 _refine_ls_number_parameters 62 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.1057 _refine_ls_wR_factor_gt 0.1037 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.0000 0.32331(4) 0.2500 0.03236(18) Uani 1 2 d S . . H1 H 0.0947(15) 0.3953(14) 0.1691(18) 0.062(5) Uiso 1 1 d . . . N1 N -0.11557(9) 0.29375(10) 0.06585(10) 0.0387(3) Uani 1 1 d . . . N2 N 0.0000 0.16852(12) 0.2500 0.0440(4) Uani 1 2 d S . . C1 C -0.04162(14) 0.27670(18) -0.06437(14) 0.0622(5) Uani 1 1 d . . . H1B H -0.0934 0.2480 -0.1421 0.093 Uiso 1 1 calc R . . H1C H 0.0230 0.2216 -0.0443 0.093 Uiso 1 1 calc R . . H1D H -0.0053 0.3491 -0.0934 0.093 Uiso 1 1 calc R . . C2 C -0.20665(13) 0.38249(14) 0.03792(19) 0.0583(4) Uani 1 1 d . . . H2A H -0.2602 0.3583 -0.0405 0.087 Uiso 1 1 calc R . . H2B H -0.1654 0.4530 0.0108 0.087 Uiso 1 1 calc R . . H2C H -0.2550 0.3953 0.1249 0.087 Uiso 1 1 calc R . . C3 C -0.17764(12) 0.18705(12) 0.10669(15) 0.0456(3) Uani 1 1 d . . . H3A H -0.2179 0.1537 0.0214 0.055 Uiso 1 1 calc R . . H3B H -0.2408 0.2030 0.1798 0.055 Uiso 1 1 calc R . . C4 C -0.08577(15) 0.10402(12) 0.16668(18) 0.0559(4) Uani 1 1 d . . . H4A H -0.1268 0.0471 0.2280 0.067 Uiso 1 1 calc R . . H4B H -0.0437 0.0639 0.0875 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0349(3) 0.0321(3) 0.0301(3) 0.000 0.00409(18) 0.000 N1 0.0325(5) 0.0548(6) 0.0289(5) 0.0030(4) 0.0028(4) 0.0086(4) N2 0.0513(9) 0.0326(7) 0.0483(9) 0.000 -0.0181(7) 0.000 C1 0.0419(7) 0.1165(14) 0.0281(6) 0.0001(7) 0.0030(5) 0.0130(9) C2 0.0453(8) 0.0695(10) 0.0601(9) 0.0138(7) -0.0038(7) 0.0172(7) C3 0.0407(7) 0.0559(8) 0.0402(7) -0.0073(5) -0.0077(5) -0.0033(5) C4 0.0651(9) 0.0411(7) 0.0614(9) -0.0110(6) -0.0214(7) -0.0010(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N2 1.8240(15) . ? Al1 N1 2.1609(10) . ? Al1 N1 2.1609(10) 3 ? Al1 H1 1.540(17) . ? N1 C2 1.4710(16) . ? N1 C1 1.4726(16) . ? N1 C3 1.4802(18) . ? N2 C4 1.4380(15) 3 ? N2 C4 1.4380(15) . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C1 H1D 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.513(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Al1 N1 80.72(3) . . ? N2 Al1 N1 80.72(3) . 3 ? N1 Al1 N1 161.44(6) . 3 ? N2 Al1 H1 123.4(6) . . ? N1 Al1 H1 95.7(6) . . ? N1 Al1 H1 94.5(6) 3 . ? C2 N1 C1 109.12(11) . . ? C2 N1 C3 109.59(11) . . ? C1 N1 C3 110.47(12) . . ? C2 N1 Al1 115.19(9) . . ? C1 N1 Al1 110.45(8) . . ? C3 N1 Al1 101.81(7) . . ? C4 N2 C4 116.17(16) 3 . ? C4 N2 Al1 121.91(8) 3 . ? C4 N2 Al1 121.91(8) . . ? N1 C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? H1B C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 109.65(11) . . ? N1 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? N1 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? N2 C4 C3 107.14(11) . . ? N2 C4 H4A 110.3 . . ? C3 C4 H4A 110.3 . . ? N2 C4 H4B 110.3 . . ? C3 C4 H4B 110.3 . . ? H4A C4 H4B 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Al1 N1 C2 150.79(9) . . . . ? N1 Al1 N1 C2 150.80(9) 3 . . . ? N2 Al1 N1 C1 -85.03(10) . . . . ? N1 Al1 N1 C1 -85.03(10) 3 . . . ? N2 Al1 N1 C3 32.31(7) . . . . ? N1 Al1 N1 C3 32.31(7) 3 . . . ? N1 Al1 N2 C4 165.98(9) . . . 3 ? N1 Al1 N2 C4 -14.02(9) 3 . . 3 ? N1 Al1 N2 C4 -14.02(9) . . . . ? N1 Al1 N2 C4 165.98(9) 3 . . . ? C2 N1 C3 C4 -167.62(12) . . . . ? C1 N1 C3 C4 72.11(14) . . . . ? Al1 N1 C3 C4 -45.21(12) . . . . ? C4 N2 C4 C3 171.64(15) 3 . . . ? Al1 N2 C4 C3 -8.36(15) . . . . ? N1 C3 C4 N2 37.69(16) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.183 _refine_diff_density_min -0.153 _refine_diff_density_rms 0.035 # Attachment 'H2Al(NL2)AlH3.cif' data_05261 _database_code_depnum_ccdc_archive 'CCDC 608296' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 05261 _chemical_melting_point ? _chemical_formula_moiety 'C8 H25 Al2 N3' _chemical_formula_sum 'C8 H25 Al2 N3' _chemical_formula_weight 217.27 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.2051(7) _cell_length_b 12.9197(14) _cell_length_c 17.4921(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1402.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3332 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.029 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 0.178 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9485 _exptl_absorpt_correction_T_max 0.9652 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans per phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16687 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.51 _reflns_number_total 3207 _reflns_number_gt 3022 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+0.1058P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(13) _refine_ls_number_reflns 3207 _refine_ls_number_parameters 137 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0718 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.76441(6) 0.56851(3) 0.03957(2) 0.02458(10) Uani 1 1 d D . . H1D H 0.646(2) 0.6418(11) -0.0115(8) 0.029 Uiso 1 1 d D . . H1E H 1.0055(18) 0.5589(11) 0.0384(8) 0.029 Uiso 1 1 d D . . Al2 Al 0.79904(8) 0.39054(3) 0.17657(2) 0.03897(12) Uani 1 1 d D . . H2D H 0.904(3) 0.3085(11) 0.1276(9) 0.047 Uiso 1 1 d D . . H2E H 0.655(2) 0.3682(13) 0.2447(8) 0.047 Uiso 1 1 d D . . H2F H 0.977(2) 0.4584(12) 0.2084(10) 0.047 Uiso 1 1 d D . . N1 N 0.7075(2) 0.44544(8) -0.04450(6) 0.0335(3) Uani 1 1 d . . . N2 N 0.61071(17) 0.47561(8) 0.10950(6) 0.0270(2) Uani 1 1 d . . . N3 N 0.74208(19) 0.67807(8) 0.13270(6) 0.0288(2) Uani 1 1 d . . . C1 C 0.9071(3) 0.40892(14) -0.08113(10) 0.0524(4) Uani 1 1 d . . . H1A H 0.8743 0.3500 -0.1145 0.079 Uiso 1 1 calc R . . H1B H 1.0100 0.3874 -0.0417 0.079 Uiso 1 1 calc R . . H1C H 0.9698 0.4650 -0.1116 0.079 Uiso 1 1 calc R . . C2 C 0.5581(4) 0.48195(14) -0.10492(10) 0.0553(5) Uani 1 1 d . . . H2A H 0.5311 0.4257 -0.1412 0.083 Uiso 1 1 calc R . . H2B H 0.6228 0.5408 -0.1319 0.083 Uiso 1 1 calc R . . H2C H 0.4218 0.5035 -0.0816 0.083 Uiso 1 1 calc R . . C3 C 0.6040(3) 0.36030(11) -0.00098(9) 0.0394(3) Uani 1 1 d . . . H3A H 0.7158 0.3138 0.0202 0.047 Uiso 1 1 calc R . . H3B H 0.5105 0.3193 -0.0354 0.047 Uiso 1 1 calc R . . C4 C 0.4713(2) 0.40524(11) 0.06315(9) 0.0393(3) Uani 1 1 d . . . H4A H 0.3477 0.4443 0.0420 0.047 Uiso 1 1 calc R . . H4B H 0.4143 0.3489 0.0958 0.047 Uiso 1 1 calc R . . C5 C 0.4723(2) 0.54387(11) 0.15734(9) 0.0363(3) Uani 1 1 d . . . H5A H 0.4005 0.5027 0.1977 0.044 Uiso 1 1 calc R . . H5B H 0.3598 0.5766 0.1253 0.044 Uiso 1 1 calc R . . C6 C 0.6139(2) 0.62628(11) 0.19323(8) 0.0345(3) Uani 1 1 d . . . H6A H 0.5232 0.6779 0.2200 0.041 Uiso 1 1 calc R . . H6B H 0.7117 0.5942 0.2312 0.041 Uiso 1 1 calc R . . C7 C 0.9550(3) 0.71015(13) 0.16350(10) 0.0443(4) Uani 1 1 d . . . H7A H 0.9338 0.7590 0.2057 0.066 Uiso 1 1 calc R . . H7B H 1.0390 0.7435 0.1230 0.066 Uiso 1 1 calc R . . H7C H 1.0326 0.6491 0.1822 0.066 Uiso 1 1 calc R . . C8 C 0.6281(3) 0.77251(11) 0.10591(9) 0.0454(4) Uani 1 1 d . . . H8A H 0.6206 0.8229 0.1477 0.068 Uiso 1 1 calc R . . H8B H 0.4819 0.7541 0.0897 0.068 Uiso 1 1 calc R . . H8C H 0.7066 0.8027 0.0627 0.068 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.02662(18) 0.02307(17) 0.02404(17) 0.00290(13) 0.00043(14) 0.00030(15) Al2 0.0485(3) 0.0329(2) 0.0355(2) 0.01003(17) -0.0025(2) 0.00570(19) N1 0.0455(7) 0.0278(5) 0.0272(5) -0.0002(4) -0.0046(5) 0.0003(5) N2 0.0261(5) 0.0253(5) 0.0297(5) 0.0009(4) 0.0021(4) -0.0014(4) N3 0.0329(6) 0.0240(5) 0.0295(5) -0.0006(4) 0.0003(5) 0.0025(5) C1 0.0662(11) 0.0430(9) 0.0479(9) -0.0115(7) 0.0133(8) 0.0022(8) C2 0.0833(14) 0.0444(9) 0.0383(9) -0.0028(7) -0.0273(9) 0.0006(9) C3 0.0523(9) 0.0271(6) 0.0388(7) -0.0033(6) -0.0083(7) -0.0077(6) C4 0.0355(7) 0.0353(7) 0.0472(8) 0.0005(6) -0.0018(6) -0.0125(6) C5 0.0291(7) 0.0375(8) 0.0423(8) 0.0004(6) 0.0131(6) 0.0028(6) C6 0.0384(7) 0.0349(7) 0.0300(6) -0.0021(5) 0.0086(6) 0.0067(6) C7 0.0429(8) 0.0453(8) 0.0446(9) -0.0132(7) -0.0022(7) -0.0086(7) C8 0.0635(11) 0.0293(7) 0.0436(8) 0.0009(6) 0.0038(8) 0.0159(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N2 1.9612(11) . ? Al1 N3 2.1625(11) . ? Al1 N1 2.1945(11) . ? Al1 H1D 1.495(11) . ? Al1 H1E 1.501(12) . ? Al2 N2 1.9874(12) . ? Al2 H2D 1.511(12) . ? Al2 H2E 1.519(12) . ? Al2 H2F 1.514(12) . ? N1 C1 1.472(2) . ? N1 C2 1.483(2) . ? N1 C3 1.4839(18) . ? N2 C5 1.4884(17) . ? N2 C4 1.4941(17) . ? N3 C6 1.4837(17) . ? N3 C7 1.486(2) . ? N3 C8 1.4862(17) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.508(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.517(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Al1 N3 84.24(4) . . ? N2 Al1 N1 84.04(4) . . ? N3 Al1 N1 165.64(5) . . ? N2 Al1 H1D 121.5(6) . . ? N3 Al1 H1D 90.3(6) . . ? N1 Al1 H1D 88.8(6) . . ? N2 Al1 H1E 116.3(5) . . ? N3 Al1 H1E 97.4(6) . . ? N1 Al1 H1E 95.2(6) . . ? H1D Al1 H1E 122.2(8) . . ? N2 Al2 H2D 107.9(7) . . ? N2 Al2 H2E 102.8(6) . . ? H2D Al2 H2E 124.5(10) . . ? N2 Al2 H2F 109.0(7) . . ? H2D Al2 H2F 107.5(10) . . ? H2E Al2 H2F 104.5(9) . . ? C1 N1 C2 108.52(13) . . ? C1 N1 C3 110.48(12) . . ? C2 N1 C3 109.33(13) . . ? C1 N1 Al1 112.86(10) . . ? C2 N1 Al1 110.35(9) . . ? C3 N1 Al1 105.24(8) . . ? C5 N2 C4 109.36(11) . . ? C5 N2 Al1 105.58(8) . . ? C4 N2 Al1 108.40(8) . . ? C5 N2 Al2 109.58(9) . . ? C4 N2 Al2 108.92(9) . . ? Al1 N2 Al2 114.88(5) . . ? C6 N3 C7 110.10(11) . . ? C6 N3 C8 109.88(11) . . ? C7 N3 C8 107.97(12) . . ? C6 N3 Al1 106.07(8) . . ? C7 N3 Al1 113.50(9) . . ? C8 N3 Al1 109.29(8) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 109.43(11) . . ? N1 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? N1 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? N2 C4 C3 108.77(11) . . ? N2 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? N2 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? N2 C5 C6 108.33(11) . . ? N2 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? N2 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? N3 C6 C5 109.37(11) . . ? N3 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? N3 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.2 . . ? N3 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Al1 N1 C1 -124.93(11) . . . . ? N3 Al1 N1 C1 -160.37(17) . . . . ? N2 Al1 N1 C2 113.47(12) . . . . ? N3 Al1 N1 C2 78.0(2) . . . . ? N2 Al1 N1 C3 -4.37(9) . . . . ? N3 Al1 N1 C3 -39.8(2) . . . . ? N3 Al1 N2 C5 31.02(9) . . . . ? N1 Al1 N2 C5 -140.67(9) . . . . ? N3 Al1 N2 C4 148.11(9) . . . . ? N1 Al1 N2 C4 -23.58(9) . . . . ? N3 Al1 N2 Al2 -89.82(6) . . . . ? N1 Al1 N2 Al2 98.48(6) . . . . ? N2 Al1 N3 C6 -3.82(9) . . . . ? N1 Al1 N3 C6 31.6(2) . . . . ? N2 Al1 N3 C7 117.20(10) . . . . ? N1 Al1 N3 C7 152.62(17) . . . . ? N2 Al1 N3 C8 -122.23(10) . . . . ? N1 Al1 N3 C8 -86.80(19) . . . . ? C1 N1 C3 C4 153.46(13) . . . . ? C2 N1 C3 C4 -87.19(15) . . . . ? Al1 N1 C3 C4 31.34(13) . . . . ? C5 N2 C4 C3 163.12(11) . . . . ? Al1 N2 C4 C3 48.49(13) . . . . ? Al2 N2 C4 C3 -77.15(12) . . . . ? N1 C3 C4 N2 -53.57(16) . . . . ? C4 N2 C5 C6 -170.42(11) . . . . ? Al1 N2 C5 C6 -53.99(12) . . . . ? Al2 N2 C5 C6 70.25(12) . . . . ? C7 N3 C6 C5 -147.50(12) . . . . ? C8 N3 C6 C5 93.70(13) . . . . ? Al1 N3 C6 C5 -24.32(12) . . . . ? N2 C5 C6 N3 52.31(14) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.156 _refine_diff_density_min -0.189 _refine_diff_density_rms 0.032 # Attachment 'H2Al(NL2)GaH3.cif' data_05126 _database_code_depnum_ccdc_archive 'CCDC 608297' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 05126 _chemical_melting_point ? _chemical_formula_moiety 'C8 H25 Al0.84 Ga1.16 N3' _chemical_formula_sum 'C8 H25 Al0.84 Ga1.16 N3' _chemical_formula_weight 266.85 _chemical_absolute_configuration ad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.2256(8) _cell_length_b 12.9136(15) _cell_length_c 17.444(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1402.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3534 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 2.286 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4616 _exptl_absorpt_correction_T_max 0.6578 _exptl_absorpt_process_details 'SADABS, R. Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART Platform CCD' _diffrn_measurement_method 'area detector, omega scans per phi' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13109 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0198 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.04 _reflns_number_total 2482 _reflns_number_gt 2335 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker' _computing_cell_refinement 'SAINT, Bruker' _computing_data_reduction 'SAINT, Bruker' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+0.2580P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.435(11) _refine_ls_number_reflns 2482 _refine_ls_number_parameters 142 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0237 _refine_ls_R_factor_gt 0.0204 _refine_ls_wR_factor_ref 0.0505 _refine_ls_wR_factor_gt 0.0491 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.2456(8) 0.4307(3) 0.0388(3) 0.02872(19) Uani 0.8435(18) 1 d PD A 1 Ga1 Ga 0.2420(15) 0.4306(7) 0.0365(5) 0.02872(19) Uani 0.1565(18) 1 d PD A 2 H1D H 0.366(3) 0.3611(15) -0.0093(12) 0.034 Uiso 1 1 d D . . H1E H 0.014(3) 0.4405(17) 0.0374(12) 0.034 Uiso 1 1 d D . . Ga2 Ga 0.20888(5) 0.61248(2) 0.176941(15) 0.04456(10) Uani 1 1 d D A . H2D H 0.358(3) 0.6200(16) 0.2395(11) 0.053 Uiso 1 1 d D . . H2E H 0.152(3) 0.7112(13) 0.1459(13) 0.053 Uiso 1 1 d D . . H2F H 0.027(3) 0.5502(16) 0.1975(12) 0.053 Uiso 1 1 d D . . N1 N 0.3043(3) 0.55590(14) -0.04643(10) 0.0375(4) Uani 1 1 d D . . N2 N 0.4031(3) 0.52315(14) 0.10751(10) 0.0313(4) Uani 1 1 d D . . N3 N 0.2682(3) 0.32176(12) 0.13329(9) 0.0327(4) Uani 1 1 d D . . C1 C 0.1046(5) 0.5938(2) -0.08216(15) 0.0543(7) Uani 1 1 d . A . H1A H 0.1381 0.6511 -0.1170 0.081 Uiso 1 1 calc R . . H1B H 0.0060 0.6181 -0.0422 0.081 Uiso 1 1 calc R . . H1C H 0.0369 0.5375 -0.1110 0.081 Uiso 1 1 calc R . . C2 C 0.4517(5) 0.5194(2) -0.10727(15) 0.0579(8) Uani 1 1 d . A . H2A H 0.4786 0.5757 -0.1436 0.087 Uiso 1 1 calc R . . H2B H 0.3863 0.4608 -0.1343 0.087 Uiso 1 1 calc R . . H2C H 0.5878 0.4974 -0.0842 0.087 Uiso 1 1 calc R . . C3 C 0.4086(4) 0.63965(17) -0.00212(13) 0.0414(6) Uani 1 1 d . A . H3A H 0.2980 0.6861 0.0198 0.050 Uiso 1 1 calc R . . H3B H 0.5020 0.6811 -0.0363 0.050 Uiso 1 1 calc R . . C4 C 0.5411(4) 0.59301(19) 0.06152(13) 0.0418(6) Uani 1 1 d . A . H4A H 0.6630 0.5536 0.0396 0.050 Uiso 1 1 calc R . . H4B H 0.5998 0.6486 0.0945 0.050 Uiso 1 1 calc R . . C5 C 0.5382(4) 0.45574(19) 0.15634(13) 0.0403(6) Uani 1 1 d . A . H5A H 0.6100 0.4976 0.1964 0.048 Uiso 1 1 calc R . . H5B H 0.6503 0.4218 0.1249 0.048 Uiso 1 1 calc R . . C6 C 0.3965(4) 0.37495(18) 0.19305(12) 0.0376(5) Uani 1 1 d . A . H6A H 0.4863 0.3238 0.2207 0.045 Uiso 1 1 calc R . . H6B H 0.2994 0.4083 0.2306 0.045 Uiso 1 1 calc R . . C7 C 0.0557(4) 0.2903(2) 0.16438(14) 0.0485(6) Uani 1 1 d . A . H7A H 0.0766 0.2428 0.2076 0.073 Uiso 1 1 calc R . . H7B H -0.0272 0.2555 0.1242 0.073 Uiso 1 1 calc R . . H7C H -0.0224 0.3518 0.1819 0.073 Uiso 1 1 calc R . . C8 C 0.3809(5) 0.22712(19) 0.10663(15) 0.0516(7) Uani 1 1 d . A . H8A H 0.3843 0.1760 0.1481 0.077 Uiso 1 1 calc R . . H8B H 0.5281 0.2448 0.0917 0.077 Uiso 1 1 calc R . . H8C H 0.3046 0.1980 0.0625 0.077 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al1 0.0329(3) 0.0291(3) 0.0242(3) -0.0031(2) -0.0007(2) 0.0008(2) Ga1 0.0329(3) 0.0291(3) 0.0242(3) -0.0031(2) -0.0007(2) 0.0008(2) Ga2 0.05586(17) 0.04130(14) 0.03653(14) -0.01093(12) 0.00271(12) 0.00680(12) N1 0.0493(11) 0.0347(9) 0.0284(9) -0.0010(8) 0.0044(9) 0.0011(9) N2 0.0294(9) 0.0325(10) 0.0319(10) -0.0007(8) -0.0035(8) -0.0003(8) N3 0.0373(10) 0.0310(9) 0.0298(9) -0.0003(7) -0.0015(8) 0.0032(8) C1 0.0699(17) 0.0503(16) 0.0427(14) 0.0071(12) -0.0139(12) 0.0043(13) C2 0.083(2) 0.0508(17) 0.0396(15) 0.0006(13) 0.0234(15) 0.0018(15) C3 0.0524(14) 0.0345(12) 0.0373(12) 0.0024(10) 0.0061(11) -0.0099(10) C4 0.0395(12) 0.0420(14) 0.0440(13) 0.0001(11) 0.0036(10) -0.0094(11) C5 0.0325(11) 0.0442(14) 0.0444(14) 0.0004(11) -0.0119(10) 0.0031(10) C6 0.0437(12) 0.0407(13) 0.0285(11) 0.0019(10) -0.0096(9) 0.0078(10) C7 0.0474(14) 0.0539(15) 0.0441(15) 0.0114(13) 0.0041(12) -0.0076(12) C8 0.0721(18) 0.0330(13) 0.0498(14) 0.0001(11) -0.0024(14) 0.0158(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al1 N2 1.956(4) . ? Al1 N3 2.171(6) . ? Al1 N1 2.227(6) . ? Al1 H1D 1.441(18) . ? Al1 H1E 1.449(18) . ? Ga1 N2 1.992(5) . ? Ga1 N3 2.202(10) . ? Ga1 N1 2.205(10) . ? Ga1 H1D 1.430(18) . ? Ga1 H1E 1.426(18) . ? Ga2 N2 2.0638(19) . ? Ga2 H2D 1.438(15) . ? Ga2 H2E 1.430(15) . ? Ga2 H2F 1.434(15) . ? N1 C1 1.474(3) . ? N1 C3 1.480(3) . ? N1 C2 1.480(3) . ? N2 C5 1.480(3) . ? N2 C4 1.482(3) . ? N3 C6 1.482(3) . ? N3 C8 1.484(3) . ? N3 C7 1.486(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.508(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.509(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Al1 N3 84.13(17) . . ? N2 Al1 N1 83.30(17) . . ? N3 Al1 N1 165.1(2) . . ? N2 Al1 H1D 118.5(9) . . ? N3 Al1 H1D 90.3(9) . . ? N1 Al1 H1D 88.8(9) . . ? N2 Al1 H1E 117.1(9) . . ? N3 Al1 H1E 97.7(9) . . ? N1 Al1 H1E 95.1(9) . . ? H1D Al1 H1E 124.4(12) . . ? N2 Ga1 N3 82.5(3) . . ? N2 Ga1 N1 83.1(3) . . ? N3 Ga1 N1 163.4(4) . . ? N2 Ga1 H1D 116.9(10) . . ? N3 Ga1 H1D 89.3(10) . . ? N1 Ga1 H1D 89.9(10) . . ? N2 Ga1 H1E 116.2(10) . . ? N3 Ga1 H1E 97.1(10) . . ? N1 Ga1 H1E 96.7(10) . . ? H1D Ga1 H1E 126.9(13) . . ? N2 Ga2 H2D 96.0(10) . . ? N2 Ga2 H2E 114.9(10) . . ? H2D Ga2 H2E 112.8(9) . . ? N2 Ga2 H2F 107.2(10) . . ? H2D Ga2 H2F 111.0(9) . . ? H2E Ga2 H2F 113.6(9) . . ? C1 N1 C3 110.40(19) . . ? C1 N1 C2 109.0(2) . . ? C3 N1 C2 109.6(2) . . ? C1 N1 Ga1 111.9(3) . . ? C3 N1 Ga1 105.70(19) . . ? C2 N1 Ga1 110.2(3) . . ? C1 N1 Al1 112.64(19) . . ? C3 N1 Al1 104.73(15) . . ? C2 N1 Al1 110.41(19) . . ? Ga1 N1 Al1 1.0(2) . . ? C5 N2 C4 109.87(18) . . ? C5 N2 Al1 106.2(2) . . ? C4 N2 Al1 109.3(2) . . ? C5 N2 Ga1 106.9(3) . . ? C4 N2 Ga1 108.7(3) . . ? Al1 N2 Ga1 0.8(5) . . ? C5 N2 Ga2 108.90(14) . . ? C4 N2 Ga2 108.49(14) . . ? Al1 N2 Ga2 114.05(18) . . ? Ga1 N2 Ga2 113.9(3) . . ? C6 N3 C8 110.32(18) . . ? C6 N3 C7 110.47(17) . . ? C8 N3 C7 108.1(2) . . ? C6 N3 Al1 105.59(15) . . ? C8 N3 Al1 109.02(19) . . ? C7 N3 Al1 113.36(19) . . ? C6 N3 Ga1 106.45(19) . . ? C8 N3 Ga1 108.7(3) . . ? C7 N3 Ga1 112.8(3) . . ? Al1 N3 Ga1 0.9(2) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 109.43(19) . . ? N1 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? N1 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.2 . . ? N2 C4 C3 108.93(18) . . ? N2 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? N2 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? N2 C5 C6 108.57(18) . . ? N2 C5 H5A 110.0 . . ? C6 C5 H5A 110.0 . . ? N2 C5 H5B 110.0 . . ? C6 C5 H5B 110.0 . . ? H5A C5 H5B 108.4 . . ? N3 C6 C5 109.70(17) . . ? N3 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? N3 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? N3 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ga1 N1 C1 -125.4(3) . . . . ? N3 Ga1 N1 C1 -155.2(16) . . . . ? N2 Ga1 N1 C3 -5.2(4) . . . . ? N3 Ga1 N1 C3 -35.0(18) . . . . ? N2 Ga1 N1 C2 113.2(3) . . . . ? N3 Ga1 N1 C2 83.3(17) . . . . ? N2 Ga1 N1 Al1 13(23) . . . . ? N3 Ga1 N1 Al1 -17(21) . . . . ? N2 Al1 N1 C1 -124.9(2) . . . . ? N3 Al1 N1 C1 -157.3(9) . . . . ? N2 Al1 N1 C3 -4.9(2) . . . . ? N3 Al1 N1 C3 -37.3(10) . . . . ? N2 Al1 N1 C2 113.0(2) . . . . ? N3 Al1 N1 C2 80.6(10) . . . . ? N2 Al1 N1 Ga1 -167(23) . . . . ? N3 Al1 N1 Ga1 161(24) . . . . ? N3 Al1 N2 C5 30.2(2) . . . . ? N1 Al1 N2 C5 -141.89(17) . . . . ? N3 Al1 N2 C4 148.63(17) . . . . ? N1 Al1 N2 C4 -23.4(2) . . . . ? N3 Al1 N2 Ga1 -169(34) . . . . ? N1 Al1 N2 Ga1 19(34) . . . . ? N3 Al1 N2 Ga2 -89.74(17) . . . . ? N1 Al1 N2 Ga2 98.20(16) . . . . ? N3 Ga1 N2 C5 30.1(3) . . . . ? N1 Ga1 N2 C5 -141.6(2) . . . . ? N3 Ga1 N2 C4 148.7(2) . . . . ? N1 Ga1 N2 C4 -23.0(4) . . . . ? N3 Ga1 N2 Al1 11(34) . . . . ? N1 Ga1 N2 Al1 -161(34) . . . . ? N3 Ga1 N2 Ga2 -90.2(3) . . . . ? N1 Ga1 N2 Ga2 98.0(3) . . . . ? N2 Al1 N3 C6 -3.0(2) . . . . ? N1 Al1 N3 C6 29.4(10) . . . . ? N2 Al1 N3 C8 -121.5(2) . . . . ? N1 Al1 N3 C8 -89.2(10) . . . . ? N2 Al1 N3 C7 118.1(2) . . . . ? N1 Al1 N3 C7 150.4(9) . . . . ? N2 Al1 N3 Ga1 171(28) . . . . ? N1 Al1 N3 Ga1 -157(29) . . . . ? N2 Ga1 N3 C6 -2.8(4) . . . . ? N1 Ga1 N3 C6 27.0(18) . . . . ? N2 Ga1 N3 C8 -121.6(3) . . . . ? N1 Ga1 N3 C8 -91.8(17) . . . . ? N2 Ga1 N3 C7 118.5(3) . . . . ? N1 Ga1 N3 C7 148.4(16) . . . . ? N2 Ga1 N3 Al1 -9(28) . . . . ? N1 Ga1 N3 Al1 21(27) . . . . ? C1 N1 C3 C4 153.17(19) . . . . ? C2 N1 C3 C4 -86.8(2) . . . . ? Ga1 N1 C3 C4 32.0(3) . . . . ? Al1 N1 C3 C4 31.7(2) . . . . ? C5 N2 C4 C3 164.88(19) . . . . ? Al1 N2 C4 C3 48.8(3) . . . . ? Ga1 N2 C4 C3 48.2(4) . . . . ? Ga2 N2 C4 C3 -76.17(19) . . . . ? N1 C3 C4 N2 -54.0(2) . . . . ? C4 N2 C5 C6 -171.40(19) . . . . ? Al1 N2 C5 C6 -53.3(3) . . . . ? Ga1 N2 C5 C6 -53.6(4) . . . . ? Ga2 N2 C5 C6 69.90(19) . . . . ? C8 N3 C6 C5 92.8(2) . . . . ? C7 N3 C6 C5 -147.80(19) . . . . ? Al1 N3 C6 C5 -24.9(2) . . . . ? Ga1 N3 C6 C5 -25.0(3) . . . . ? N2 C5 C6 N3 52.3(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.267 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.039